CN110040740A - The method that crystal seed is oriented to method synthesis total silicon SOD zeolite - Google Patents
The method that crystal seed is oriented to method synthesis total silicon SOD zeolite Download PDFInfo
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- CN110040740A CN110040740A CN201910384748.9A CN201910384748A CN110040740A CN 110040740 A CN110040740 A CN 110040740A CN 201910384748 A CN201910384748 A CN 201910384748A CN 110040740 A CN110040740 A CN 110040740A
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- crystal seed
- sod
- total silicon
- silicon
- zeolite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/06—Preparation of isomorphous zeolites characterised by measures to replace the aluminium or silicon atoms in the lattice framework by atoms of other elements, i.e. by direct or secondary synthesis
- C01B39/08—Preparation of isomorphous zeolites characterised by measures to replace the aluminium or silicon atoms in the lattice framework by atoms of other elements, i.e. by direct or secondary synthesis the aluminium atoms being wholly replaced
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The present invention relates to molecular sieve preparation methods, it is desirable to provide a kind of method of crystal seed guiding method synthesis total silicon SOD zeolite.Include: to take silicon source, alkali source and ethyl alcohol, mixes to be placed in mortar with total silicon SOD crystal seed and grind；Then it goes in reaction kettle, 1~7d of crystallization at 100~155 DEG C；Product is filtered, is dried to get total silicon SOD zeolite is arrived.The present invention only uses nontoxic ethyl alcohol as duct filler, is oriented to using crystal seed, avoids using virose organic matter；The yield of product can be greatly improved, and synthetic operation is simple and easy.Water is added without in synthetic system, reaction process keeps solid state shape, reduces unnecessary waste discharge and loss.Product keeps crystallinity and purity, has good reactivity.Used inorganic raw material is environmentally friendly, and price is less expensive, thus is of great significance in practical chemical production field.
Description
Technical field
The invention belongs to molecular sieve preparation methods, more particularly to the method for crystal seed guiding method synthesis total silicon SOD zeolite.
Background technique
Hexatomic ring SOD pore zeolite is widely used for the fields such as catalyst carrier, adsorbing separation, semiconductor, pigment, thus
Receive the extensive concern of researcher in recent years.The sieve and silica-sesquioxide ratio of usual SOD zeolite is 2, in organic-free template
Under the conditions of can synthesize.But the SOD zeolite of the even total silicon for high silicon, it usually needs organic matter is carried out as template
Filling is to synthesize.At this stage, the synthesis of total silicon SOD zeolite is needed using this nitrogenous template of pyrrolidines.Usually this
The nitrogenous template strong toxicity of class, pollution weight, irritant ammonia odor, this is unfavorable for the synthesis of total silicon SOD zeolite.This
Outside, glycerine and this polyalcohol template of ethylene glycol has been developed to carry out the synthesis of total silicon SOD zeolite.Although substantially reducing
The toxicity of template.But these polyalcohol boiling points are high, it is not easy to separate from waste liquid.Certainly, still have a bit
Toxicity.
Therefore, it needs to develop synthesis of the nontoxic and pollution-free route of one kind to carry out total silicon SOD zeolite.
Summary of the invention
The technical problem to be solved by the present invention is to overcome deficiency in the prior art, provide a kind of crystal seed guiding method synthesis
The method of total silicon SOD zeolite.
In order to solve the technical problem, solution of the invention is:
A kind of method of crystal seed guiding method synthesis total silicon SOD zeolite is provided, comprising the following steps:
By SiO2∶Na2O: the molar ratio of ethyl alcohol is 1: 0.04~0.11: 0.4~1.5 to take silicon source, alkali source and ethyl alcohol, and complete
The mixing of silicon SOD crystal seed, which is placed in mortar, grinds；Then it goes in reaction kettle, 1~7d of crystallization at 100~155 DEG C；It will
Product is filtered, is dried to get total silicon SOD zeolite is arrived.
In the present invention, the total silicon SOD crystal seed accounts for SiO in silicon source2The 1~10% of quality.
In the present invention, the silicon source is solid silicone or white carbon black.
In the present invention, the alkali source is sodium hydroxide or sodium metasilicate.
Compared with prior art, the beneficial effects of the present invention are:
1, the present invention only uses nontoxic ethyl alcohol as duct filler, is oriented to using crystal seed, thus is avoided that use
Virose organic matter；
2, the method for the present invention greatly improves the yield (being promoted by the 85% of traditional technology to 98.6%) of product, and
Synthetic operation is simple and easy.
3, water is added without in synthetic system of the invention, reaction process keeps solid state shape, reduces unnecessary waste
Discharge and loss.
4, total silicon SOD zeolite made from this method maintains crystallinity and purity, has good reactivity.
5, inorganic raw material of the present invention is environmentally friendly, and price is less expensive, thus leads in practical Chemical Manufacture
Domain is of great significance.
Detailed description of the invention
Fig. 1 is the XRD spectra for the total silicon SOD zeolite that the present invention synthesizes.
Fig. 2 is the SEM photograph for the total silicon SOD zeolite that the present invention synthesizes.
Specific embodiment
Embodiment 1: crystal seed is oriented to method and synthesizes total silicon SOD zeolite
By 0.53g Na2SiO3·9H2O, 1.56g solid silicone, 1.9g ethyl alcohol and the 0.035g total silicon as crystal seed
SOD (account in silicon source silica quality than 2%) crystal seed, which is placed in grinding, to be ground, and then crystallization 3d can be complete at 140 DEG C
Crystallization, product filter, and total silicon SOD zeolite product is obtained after drying.
The molar ratio of each reaction raw materials is as follows:
SiO2∶Na2O: ethyl alcohol=1: 0.07: 1.5
Obtaining its structure by XRD analysis is total silicon SOD zeolite (Fig. 1), and finds out that the method obtains by SEM photograph
Total silicon SOD zeolite be the bulk morphologies (Fig. 2) with aggregate.
Embodiment 2: crystal seed guiding method synthesizes total silicon SOD zeolite under relatively-high temperature
By 0.32g Na2SiO3·9H2O, 1.63g solid silicone, 0.95g ethyl alcohol and the 0.17g total silicon as crystal seed
SOD (account in silicon source silica quality than 10%) crystal seed, which is placed in grinding, to be ground, and then crystallization 1d can be complete at 155 DEG C
Crystallization, product filter, and total silicon SOD zeolite product is obtained after drying.
The molar ratio of each reaction raw materials is as follows:
SiO2∶Na2O: ethyl alcohol=1: 0.04: 0.75
Embodiment 3: crystal seed guiding method synthesizes total silicon SOD zeolite under relative low temperature
By 0.85g Na2SiO3·9H2O, 1.39g solid silicone, 0.51g ethyl alcohol and the 0.017g total silicon as crystal seed
SOD (account in silicon source silica quality than 1%) crystal seed, which is placed in grinding, to be ground, and then crystallization 7d can be complete at 100 DEG C
Crystallization, product filter, and total silicon SOD zeolite product is obtained after drying.
The molar ratio of each reaction raw materials is as follows:
SiO2∶Na2O: ethyl alcohol=1: 0.11: 0.4
Embodiment 4: method is oriented to as alkali source crystal seed using NaOH and synthesizes total silicon SOD zeolite
0.12g NaOH, 1.67g solid silicone, 0.95g ethyl alcohol and 0.17g total silicon SOD as crystal seed (are accounted for into silicon source
Middle silica quality than 10%) crystal seed be placed in grinding in grind, then at 140 DEG C crystallization 4d can complete crystallization, product
It filters, total silicon SOD zeolite product is obtained after drying.
The molar ratio of each reaction raw materials is as follows:
SiO2∶Na2O: ethyl alcohol=1: 0.05: 0.75
Embodiment 5: method is oriented to as silicon source crystal seed using white carbon black and synthesizes total silicon SOD zeolite
By 0.53g Na2SiO3·9H2O, 1.55g white carbon black, 1.43g ethyl alcohol and the 0.035g total silicon SOD as crystal seed
(account in silicon source silica quality than 2%) crystal seed is placed in grinding and grinds, and then crystallization 3d can be completely brilliant at 140 DEG C
Change, product filters, and total silicon SOD zeolite product is obtained after drying.
The molar ratio of each reaction raw materials is as follows:
SiO2∶Na2O: ethyl alcohol=1: 0.07: 1.1
The above is only several case study on implementation of the invention, not does limitation in any form to the present invention,
Although the present invention is disclosed as above with preferable case study on implementation, however, it is not intended to limit the invention, any skill for being familiar with this profession
Art personnel, without departing from the scope of the present invention, when the structure and technology contents using the disclosure above make it is a little
Change or be modified to the equivalence enforcement case of equivalent variations.But anything that does not depart from the technical scheme of the invention, foundation
Technical spirit of the invention still belongs to the present invention to any simple modification, equivalent change and modification made by the above case study on implementation
In technical proposal scope.
Claims (4)
1. a kind of method of crystal seed guiding method synthesis total silicon SOD zeolite, which comprises the following steps:
By SiO2∶Na2O: the molar ratio of ethyl alcohol takes silicon source, alkali source and ethyl alcohol for 1: 0.04~0.11: 0.4~1.5, with total silicon SOD
Crystal seed mixing, which is placed in mortar, grinds；Then it goes in reaction kettle, 1~7d of crystallization at 100~155 DEG C；By product
It filters, dry to get total silicon SOD zeolite is arrived.
2. the method according to claim 1, wherein the total silicon SOD crystal seed accounts for SiO in silicon source2The 1 of quality~
10%.
3. the method according to claim 1, wherein the silicon source is solid silicone or white carbon black.
4. the method according to claim 1, wherein the alkali source is sodium hydroxide or sodium metasilicate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111634923A (en) * | 2020-05-15 | 2020-09-08 | 浙江大学 | Method for synthesizing FER molecular sieve by using alcohol as organic template agent |
| CN112570015A (en) * | 2020-12-22 | 2021-03-30 | 天津大学 | Molecular sieve catalyst for packaging Pd-based alloy and preparation method and application thereof |
Citations (6)
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|---|---|---|---|---|
| CN103964462A (en) * | 2014-05-19 | 2014-08-06 | 吉林大学 | Method for quickly synthesizing zeolite molecular sieve by microwave solid-phase method |
| CN106256764A (en) * | 2015-06-19 | 2016-12-28 | 中国石油化工股份有限公司 | A kind of method preparing the molecular sieve molded thing of nanoscale sodalite |
| CN108190913A (en) * | 2018-03-02 | 2018-06-22 | 浙江大学 | The method of method synthesis Silicon-rich ZSM-5 zeolite molecular sieve is oriented to using crystal seed |
| CN108217682A (en) * | 2018-03-02 | 2018-06-29 | 浙江大学 | The method of method synthesis Silicon-rich ZSM-48 zeolite molecular sieves is oriented to using crystal seed |
| CN108217683A (en) * | 2018-03-02 | 2018-06-29 | 浙江大学 | The method of method synthesis Silicon-rich ZSM-23 zeolite molecular sieves is oriented to using crystal seed |
| CN109160522A (en) * | 2018-09-06 | 2019-01-08 | 嘉兴学院 | A kind of method of solvent-free solid-phase synthesis total silicon SOD zeolite |
-
2019
- 2019-05-09 CN CN201910384748.9A patent/CN110040740A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103964462A (en) * | 2014-05-19 | 2014-08-06 | 吉林大学 | Method for quickly synthesizing zeolite molecular sieve by microwave solid-phase method |
| CN106256764A (en) * | 2015-06-19 | 2016-12-28 | 中国石油化工股份有限公司 | A kind of method preparing the molecular sieve molded thing of nanoscale sodalite |
| CN108190913A (en) * | 2018-03-02 | 2018-06-22 | 浙江大学 | The method of method synthesis Silicon-rich ZSM-5 zeolite molecular sieve is oriented to using crystal seed |
| CN108217682A (en) * | 2018-03-02 | 2018-06-29 | 浙江大学 | The method of method synthesis Silicon-rich ZSM-48 zeolite molecular sieves is oriented to using crystal seed |
| CN108217683A (en) * | 2018-03-02 | 2018-06-29 | 浙江大学 | The method of method synthesis Silicon-rich ZSM-23 zeolite molecular sieves is oriented to using crystal seed |
| CN109160522A (en) * | 2018-09-06 | 2019-01-08 | 嘉兴学院 | A kind of method of solvent-free solid-phase synthesis total silicon SOD zeolite |
Non-Patent Citations (2)
| Title |
|---|
| YAO JIANFENG ET AL.: "Synthesis of nanocrystalline sodalite with organic additives", 《MATERIALS LETTERS》 * |
| ZHANG SHAOQING ET AL.: "Study on the synthesis of FER and SOD in the presence of ethylene glycol and the oxidation transformation of ethylene glycol in a confined region of zeolites", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111634923A (en) * | 2020-05-15 | 2020-09-08 | 浙江大学 | Method for synthesizing FER molecular sieve by using alcohol as organic template agent |
| CN111634923B (en) * | 2020-05-15 | 2022-02-08 | 浙江大学 | Method for synthesizing FER molecular sieve by using alcohol as organic template agent |
| CN112570015A (en) * | 2020-12-22 | 2021-03-30 | 天津大学 | Molecular sieve catalyst for packaging Pd-based alloy and preparation method and application thereof |
| CN112570015B (en) * | 2020-12-22 | 2022-08-26 | 天津大学 | Molecular sieve catalyst for packaging Pd-based alloy and preparation method and application thereof |
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